EP1584921A1 - Keramisches Heizelement für Gassensoren - Google Patents
Keramisches Heizelement für Gassensoren Download PDFInfo
- Publication number
- EP1584921A1 EP1584921A1 EP05101156A EP05101156A EP1584921A1 EP 1584921 A1 EP1584921 A1 EP 1584921A1 EP 05101156 A EP05101156 A EP 05101156A EP 05101156 A EP05101156 A EP 05101156A EP 1584921 A1 EP1584921 A1 EP 1584921A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- heating element
- barium
- substance
- ceramic
- ceramic heating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/403—Cells and electrode assemblies
- G01N27/406—Cells and probes with solid electrolytes
- G01N27/4067—Means for heating or controlling the temperature of the solid electrolyte
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
- H05B3/26—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base
- H05B3/265—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base the insulating base being an inorganic material, e.g. ceramic
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
- H05B3/28—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material
- H05B3/283—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material the insulating material being an inorganic material, e.g. ceramic
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/022—Heaters specially adapted for heating gaseous material
Definitions
- the invention relates to a ceramic heating element and a method for the same Manufacture according to the type defined in the preamble of the independent claims.
- Ceramic gas sensors based on solid electrolytes for determining the concentration of Gases in gas mixtures have multiple electrodes, to determine the Gas concentration the potential difference between the electrodes, one between the Electrodes flowing pumping current or the electrical resistance of the between the Electrodes located solid electrolyte material is used. Furthermore, such Gas sensors on at least one ceramic heating element, since the ceramic Solid electrolyte material of the sensors only at operating temperatures of more than 400 ° C a has sufficient ionic conductivity. Usually, the ceramic heating elements composed of two insulating layers, between which an electrically conductive Resistor track is located when applying a corresponding heating voltage strongly heated. Due to operational reasons, comparatively flow through the resistor track big streams.
- the object of the present invention is to provide a ceramic heating element which shows only slight couplings in the measuring signals of the underlying gas sensor and yet long-term stable.
- the ceramic heating element with the features of claim 1 has the advantage that it so is carried out that coupling the heating voltage in measuring signals of a corresponding Gas sensor can be avoided and the material structure of the ceramic heating element nevertheless has a good long-term stability.
- the substance forms advantageously with the diffusing into the resistance track barium a chemical stable compound, such as a corresponding mixed oxide, whereby a Reaction of barium oxide with the metallic part (s) of the resistance trace is prevented with formation of binary mixed oxides.
- the substance is a metal oxide, wherein the metal oxide with barium forms a mixed oxide.
- the resulting binary or ternary metal oxides provide particularly stable chemical compounds; thus becomes diffusing barium tied particularly effectively. This is especially true when doing a binary or ternary Mixed oxide is produced, which is more stable than a mixed oxide formed from barium oxide and metallic Shares of the resistance track.
- the substance is a titanium oxide, zirconium dioxide, hafnium dioxide or silica, since these form particularly stable mixed oxides with barium.
- Farther Tantalum pentoxide or niobium pentoxide are also suitable as a substance.
- the ceramic heating element is the Substance in the resistance conductor track in a concentration of 100 to 50,000 ppm contained in the content of titanium, zirconium, hafnium, silicon, tantalum or niobium.
- FIG. 1 shows a vertical longitudinal section through a ceramic Heating element according to one embodiment
- Figures 2 and 3 show the Thermodynamic stability of various barium mixed oxides at 1200 Kelvin depending their composition in diagram form
- Figures 4 to 6 show phase diagrams corresponding barium mixed oxides.
- FIG. 1 shows a basic structure of a first embodiment of the present invention shown.
- a ceramic heating element is, for example, an electrochemical Gas sensors called.
- the ceramic heating element 10 preferably has a first one electrically insulating ceramic layer 21, for example, from a barium-containing Alumina are executed.
- the ceramic heating element 10 also has a further insulation layer 13, which in addition to the insulating layer 18 two further ceramic Layers 14, 15 comprises.
- the insulating layer 18 is for example also made of a Barium-containing alumina carried out.
- the further ceramic layers 14, 15 are only optionally provided to intercept mechanical or ceramic stresses, if necessary, which may occur when the ceramic heating element 10 in a corresponding Sensor element is integrated and follow the sequence of layers 18, 15, 14, for example connect ceramic solid electrolyte layers of a sensor element.
- the further layers 14, 15 are preferably made of a mixture of the ceramic Material of which the insulating layer 18 and the insulating layer 21 consists and the performed ceramic material of the solid electrolyte layers of a sensor element.
- the ceramic layers 14, 15 may have a similar composition. she include, for example, the ceramic material of the insulating layer 18 and the Solid electrolyte material in a ratio of 1: 1.
- Another possibility is the further layer 15 predominantly of the ceramic material of the insulating layer 18th and the further layer 14 of a material with a higher proportion Solid electrolyte material.
- the further layer 15 the material of insulating layer 18 in a ratio to the solid electrolyte content of 70: 30 included and the further layer 14 the material of the insulating layer 18 in relation to Solid electrolyte content of 30: 70.
- the ceramic heating element 10 further comprises an electrically conductive, metal-containing Resistance conductor 19, which serves to heat the ceramic heating element 10.
- the Resistance conductor 19 is preferably designed in the form of a meander and has both ends not shown electrical connections. By creating a corresponding heating voltage to the terminals of the resistor track 19, the Heating power of the heating element 10 are regulated accordingly.
- a material of the resistor track 19 is in particular a mixture of a metal, such as for example, platinum, with ceramic proportions, such as alumina, used.
- a metal such as for example, platinum
- ceramic proportions such as alumina
- the material of the Resistor conductor 19 provided as a so-called cermet and used as a printing paste.
- the integrated form of the planar ceramic heating element 10 is laminated together the printed with functional layers ceramic films and subsequent sintering the laminated structure produced in a conventional manner.
- the insulating layer 21 or the insulating layer 18, the resistor track 19 contains, to reduce their electrical conductivity, a proportion of 1 to 20 % By weight of barium oxide, preferably 5 to 10% by weight.
- barium oxide preferably 5 to 10% by weight.
- the resulting barium platinates lead to a disorder of the Material structure of the resistor track 19 and thus to a restriction of Heating power of the heating element 10 and possibly to its failure.
- the resistor track 19 contains in addition to a metallic portion in the form of platinum also alumina, which in turn forms stable mixed oxides with barium.
- the mixed oxides have in principle at high temperatures on a sufficient thermodynamic stability, so that a further reaction with the platinum of the resistor track 19 actually is excluded.
- the alumina content of the resistive trace 19 is insufficient to completely or at least largely diffuse barium intercept.
- the resistor trace 19 contains another substance, the forms a chemical compound with barium or barium oxide, wherein the forming chemical compound has a higher thermodynamic stability than those Mixed oxides, consisting of the metallic portions of the resistor track 19 with Barium oxide can form.
- FIGS. 2 and 3 exemplify the thermodynamic stabilities of some mixed oxides of Barium oxide with elements of the fourth or fifth main or subgroup in dependence their mixing ratios at 1200 K stated.
- Mixed oxides with silicon, titanium, niobium or zirconium are suitable.
- the resistance trace 19 tantalum pentoxide or niobium pentoxide in a concentration of 100 to 50,000 ppm, in particular from 2000 to 7000 ppm, based on the content of niobium or tantalum have.
- a third possibility is the addition from 100 to 10,000 ppm, especially from 300 to 2000 ppm, of a titanium oxide or of Silica, based on the content of titanium or silicon.
- barium oxide forms celsian in the presence of alumina and silica as the ternary phase.
- This reaction proceeds via the formation of mullite and is kinetically inhibited.
- niobium pentoxide is used instead of silicon dioxide as the barium scavenging substance, the formation of a ternary phase is bypassed, but a binary phase of AlNbO 4 still forms in an intermediate step.
- FIG. Another phase diagram is shown in FIG. It shows that the reaction of zirconia with barium oxide proceeds without formation of an intermediate.
- test results are listed by way of example which demonstrate the effectiveness of the Addition of a substance for trapping barium to the material of the resistor track of a heating element occupy.
- sample 1 and 2 include resistive traces of conventional material, and Samples 3 through 5 are doped with 2 weight percent Nb 2 O 5 . All samples have barium-containing ceramics as heater insulation.
- Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 0 - 8500 cycles 4:55 4.25 0.95 1:43 1.10 0 - 23000 cycles def. Def. 0.66 00:55 00:52 0 - 37800 cycles def. Def. 1:51 2:01 1:47 0 - 48500 cycles def. Def. 2.28 4.13 2.64 0 - 60000 cycles def. Def. def. def. def. def.
- the increase in electrical resistance of zirconium-containing resistive tracks is plotted at operating temperature as a function of the number of operating cycles driven. Each operating cycle involves the application of a heating voltage of 15.2 V for 9 seconds.
- Samples 1 to 3 have resistance conductors of conventional material, samples 4 to 6 are doped with 0.5% by weight of ZrO 2 . All samples contain barium-containing ceramics as heater insulation.
- Sample 1 Sample 2
- Sample 3 Sample 4 Sample 5 Sample 6 0 - 14614 cycles 2.26 1.86 1.74 00:09 00:14 -0.13 0-29244 cycles 6.17 5.81 5.11 0.97 0.87 00:41 0 - 41960 cycles def. 7.69 Def. 1.25 1:32 0.84 0 - 52600 cycles def. def. Def 2:48 2.62 2.22 0 - 67200 cycles def. def. Def. def. def. def. def.
- Samples 1 to 3 include resistive traces of conventional material, and Samples 4 to 6 are doped with 0.5% by weight of ZrO 2 . All samples have barium-containing ceramics as heater insulation.
- Sample 1 Sample 2 Sample 3
- Sample 4 Sample 5
- Sample 6 0-10600 cycles 1.28 2.11 2:42 1:45 0.84 0.86 0 - 34600 cycles 12.96 def. def. 4:47 4:57 3:47 0 - 42250 cycles def. def. def. 6:54 7.80 6:04 0 - 57500 cycles def. def. def. def. def.
Abstract
Description
Probe 1 | Probe 2 | Probe 3 | Probe 4 | Probe 5 | |
0 - 8500 Zyklen | 4.55 | 4.25 | 0.95 | 1.43 | 1.10 |
0 - 23000 Zyklen | def. | Def. | 0.66 | 0.55 | 0.52 |
0 - 37800 Zyklen | def. | Def. | 1.51 | 2.01 | 1.47 |
0 - 48500 Zyklen | def. | Def. | 2.28 | 4.13 | 2.64 |
0 - 60000 Zyklen | def. | Def. | def. | def. | def. |
Probe 1 | Probe 2 | Probe 3 | Probe 4 | Probe 5 | Probe 6 | |
0 - 14614 Zyklen | 2.26 | 1.86 | 1.74 | 0.09 | 0.14 | -0.13 |
0 - 29244 Zyklen | 6.17 | 5.81 | 5.11 | 0.97 | 0.87 | 0.41 |
0 - 41960 Zyklen | def. | 7.69 | Def. | 1.25 | 1.32 | 0.84 |
0 - 52600 Zyklen | def. | def. | Def | 2.48 | 2.62 | 2.22 |
0 - 67200 Zyklen | def. | def. | Def. | def. | def. | def. |
Probe 1 | Probe 2 | Probe 3 | Probe 4 | Probe 5 | Probe 6 | |
0 - 10600 Zyklen | 1.28 | 2.11 | 2.42 | 1.45 | 0.84 | 0.86 |
0 - 34600 Zyklen | 12.96 | def. | def. | 4.47 | 4.57 | 3.47 |
0 - 42250 Zyklen | def. | def. | def. | 6.54 | 7.80 | 6.04 |
0 - 57500 Zyklen | def. | def. | def. | def. | def. | def. |
Claims (10)
- Keramisches Heizelement für Sensoren zur Detektion eines Gases in Gasgemischen mit mindestens einer metallhaltigen Widerstandsleiterbahn (19) und mit mindestens einer Isolationsschicht (13, 21), dadurch gekennzeichnet, dass die metallische Widerstandsleiterbahn (19) zusätzlich eine Substanz enthält, die eine Reaktion von Barium mit dem oder den metallischen Anteilen der Widerstandsleiterbahn (19) verhindert.
- Keramisches Heizelement nach Anspruch 1, dadurch gekennzeichnet, dass die Substanz ein Metalloxid ist, wobei das Metalloxid mit Barium ein Mischoxid bildet, das stabiler ist als ein Mischoxid, das aus Bariumoxid und dem metallischen Anteil der Widerstandsleiterbahn (19) gebildet ist.
- Keramisches Heizelement nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Substanz ein Titanoxid, Zirconiumdioxid, Hafniumdioxid oder Siliciumdioxid ist.
- Keramisches Heizelement nach Anspruch 3, dadurch gekennzeichnet, dass die Substanz in der Widerstandsleiterbahn (19) in einer Konzentration von 100 bis 10000 ppm bezogen auf den Gehalt an Titan, Zirconium, Hafnium bzw. Silicium enthalten ist.
- Keramisches Heizelement nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Substanz Tantalpentoxid oder Niobiumpentoxid ist.
- Keramisches Heizelement nach Anspruch 5, dadurch gekennzeichnet, dass die Substanz in der Widerstandsleiterbahn (19) in einer Konzentration von 100 bis 50000 ppm bezogen auf den Gehalt an Tantal bzw. Niobium enthalten ist.
- Keramisches Heizelement nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass der metallische Anteil der Widerstandsleiterbahn (19) Platin ist.
- Keramisches Heizelement nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Widerstandsleiterbahn (19) weiterhin Aluminiumoxid enthält.
- Verfahren zur Herstellung eines keramischen Heizelements mit mindestens einer metallhaltigen Widerstandsleiterbahn (19) und mit mindestens einer Isolationsschicht (13, 21), wobei in einem ersten Schritt eine keramische Druckpaste erzeugt wird, die einen metallischen Anteil, einen keramischen Anteil und eine Substanz enthält, die eine Reaktion von Barium mit dem metallischen Anteil der Widerstandsleiterbahn verhindert, und wobei in einem zweiten Schritt auf die Isolationsschicht (13, 21) mittels der keramischen Druckpaste eine Widerstandsleiterbahn (19) gedruckt wird.
- Verfahren nach Anspruch 9, dadurch gekennzeichnet, dass als Substanz zur Verhinderung einer Reaktion von Barium mit dem metallischen Anteil der Widerstandsleiterbahn (19) eine Substanz nach einem der Ansprüche 1 bis 8 verwendet wird.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE200410016008 DE102004016008A1 (de) | 2004-04-01 | 2004-04-01 | Keramisches Heizelement für Gassensoren |
DE102004016008 | 2004-04-01 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1584921A1 true EP1584921A1 (de) | 2005-10-12 |
EP1584921B1 EP1584921B1 (de) | 2011-10-12 |
Family
ID=34895470
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP20050101156 Expired - Fee Related EP1584921B1 (de) | 2004-04-01 | 2005-02-16 | Keramisches Heizelement für Gassensoren |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP1584921B1 (de) |
JP (1) | JP4662803B2 (de) |
DE (1) | DE102004016008A1 (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2006053848A1 (de) * | 2004-11-16 | 2006-05-26 | Robert Bosch Gmbh | Keramisches isolationsmaterial sowie sensorelement dieses enthaltend |
CN109896499A (zh) * | 2019-03-04 | 2019-06-18 | 中国电子科技集团公司第四十九研究所 | 一种陶瓷微结构石墨烯气体传感器及其制造方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4798693A (en) * | 1984-04-26 | 1989-01-17 | Ngk Insulators, Ltd. | Method of manufacturing an electrochemical device |
US5773894A (en) | 1993-12-09 | 1998-06-30 | Robert Bosch Gmbh | Insulation layer system for the electrical isolation circuits |
US20020175154A1 (en) * | 2001-04-27 | 2002-11-28 | Harison Toshiba Lighting Corporation | Heater |
EP1306666A2 (de) * | 1995-03-09 | 2003-05-02 | Ngk Insulators, Ltd. | Verfahren und Vorrichtung zur Messung einer brennbaren Gaskomponente durch Verbrennung der Komponente |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH04249089A (ja) * | 1991-02-05 | 1992-09-04 | Noritake Co Ltd | セラミックスヒーター |
JP3572241B2 (ja) * | 2000-03-29 | 2004-09-29 | 京セラ株式会社 | 空燃比センサ素子 |
DE19932545A1 (de) * | 1999-07-13 | 2001-01-18 | Bosch Gmbh Robert | Heizleiter, insbesondere für einen Meßfühler, und ein Verfahren zur Herstellung des Heizleiters |
JP4689860B2 (ja) * | 2001-03-30 | 2011-05-25 | 京セラ株式会社 | ヒータ一体型酸素センサ素子 |
JP4744043B2 (ja) * | 2001-09-26 | 2011-08-10 | 京セラ株式会社 | 空燃比センサ素子 |
JP2004151017A (ja) * | 2002-10-31 | 2004-05-27 | Denso Corp | 積層型ガスセンサ素子 |
-
2004
- 2004-04-01 DE DE200410016008 patent/DE102004016008A1/de not_active Ceased
-
2005
- 2005-02-16 EP EP20050101156 patent/EP1584921B1/de not_active Expired - Fee Related
- 2005-04-01 JP JP2005106832A patent/JP4662803B2/ja not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4798693A (en) * | 1984-04-26 | 1989-01-17 | Ngk Insulators, Ltd. | Method of manufacturing an electrochemical device |
US5773894A (en) | 1993-12-09 | 1998-06-30 | Robert Bosch Gmbh | Insulation layer system for the electrical isolation circuits |
EP1306666A2 (de) * | 1995-03-09 | 2003-05-02 | Ngk Insulators, Ltd. | Verfahren und Vorrichtung zur Messung einer brennbaren Gaskomponente durch Verbrennung der Komponente |
US20020175154A1 (en) * | 2001-04-27 | 2002-11-28 | Harison Toshiba Lighting Corporation | Heater |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2006053848A1 (de) * | 2004-11-16 | 2006-05-26 | Robert Bosch Gmbh | Keramisches isolationsmaterial sowie sensorelement dieses enthaltend |
CN109896499A (zh) * | 2019-03-04 | 2019-06-18 | 中国电子科技集团公司第四十九研究所 | 一种陶瓷微结构石墨烯气体传感器及其制造方法 |
CN109896499B (zh) * | 2019-03-04 | 2021-02-09 | 中国电子科技集团公司第四十九研究所 | 一种陶瓷微结构石墨烯气体传感器及其制造方法 |
Also Published As
Publication number | Publication date |
---|---|
JP4662803B2 (ja) | 2011-03-30 |
JP2005308739A (ja) | 2005-11-04 |
DE102004016008A1 (de) | 2005-10-20 |
EP1584921B1 (de) | 2011-10-12 |
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